CN117305675A - High Wen Gaoshang alloy and preparation method and application thereof - Google Patents
High Wen Gaoshang alloy and preparation method and application thereof Download PDFInfo
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- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C30/00—Alloys containing less than 50% by weight of each constituent
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/023—Alloys based on nickel
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
- C22C19/05—Alloys based on nickel or cobalt based on nickel with chromium
- C22C19/051—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W
- C22C19/056—Alloys based on nickel or cobalt based on nickel with chromium and Mo or W with the maximum Cr content being at least 10% but less than 20%
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01D—NON-POSITIVE DISPLACEMENT MACHINES OR ENGINES, e.g. STEAM TURBINES
- F01D25/00—Component parts, details, or accessories, not provided for in, or of interest apart from, other groups
- F01D25/005—Selecting particular materials
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- General Engineering & Computer Science (AREA)
- Powder Metallurgy (AREA)
Abstract
The invention provides a high Wen Gaoshang alloy, which comprises the following elements in percentage by mass: 0.03 to 0.04wt.% of C, 4 to 5.5wt.% of W, 0.5 to 3.5wt.% of Nb, 2 to 4.5wt.% of Ti, 4 to 6wt.% of Mo, 5.5 to 8wt.% of Al, 16.5 to 19wt.% of Fe, 8 to 10wt.% of Cr, 19 to 22wt.% of Co, and the balance of Ni. The high Wen Gaoshang alloy provided by the invention forms gamma phase, gamma 'phase and TiC, and the gamma' phase is uniformly distributed on the gamma phase of the matrix as a second phase strengthening phase to form the high Wen Gaoshang alloy with the 'cocktail' effect, the high-temperature service performance of the alloy is improved on the premise of low density, and the high-temperature resistant alloy has good hot forming processing capacity and is suitable for high-temperature resistant structural members such as turbine discs of spaceflight engines.
Description
Technical Field
The invention belongs to the technical field of alloys, and particularly relates to a high Wen Gaoshang alloy and a preparation method and application thereof.
Background
The high-temperature alloy is widely applied to the fields of space engines, gas turbines, liquid rocket engines, steam turbines, heat exchanger tubes, chemical petroleum and the like as a heat-resistant material. In the case of aerospace engines, superalloy is used primarily to fabricate hot end components, such as blades, turbine disks, and the like. The turbine disk is mainly used for fixing turbine blades and is a rotating bearing piece with the greatest stress, and materials used by the turbine disk are required to have good high-temperature strength, high-temperature toughness, high-temperature oxidation resistance and tissue stability under high temperature and complex stress level. The traditional nickel-based superalloy has excellent mechanical properties and physical properties at higher service temperature, and is a main material for high-temperature-resistant structural materials such as turbine discs. However, with the progress of technology and the development of aeroengines, the service temperature of turbine disk alloys is increased, and high-temperature alloys gradually tend to be designed in a high alloying direction in order to meet the performance requirements.
Conventional superalloys are classified into iron-based superalloys, cobalt-based superalloys, and nickel-based superalloys according to the alloying matrix elements. The iron-based superalloy has low heat bearing temperature, narrow service temperature range and less application. Cobalt-based superalloys are limited in large-scale application and slow in development due to poor thermal stability and high price. The nickel-based superalloy has the largest proportion in superalloy application due to lower cost, better high-temperature stability, wide high Wen Fuyi temperature range, such as GH4169, GH4145, inconel725 and Inconel625 which are commonly used. However, along with the demands of increasing the service temperature and reducing the weight of the high-temperature structural member, the traditional nickel-based superalloy faces two major difficulties of component design and density control. Therefore, the novel high-temperature alloy structural material with low cost, high strength and breaking through the temperature limit of the nickel-based superalloy is developed, and the alloy is endowed with good hot forming processing behavior, so that the novel high-temperature alloy structural material has important engineering application value and scientific significance.
The high-entropy alloy is influenced by four effects such as high entropy effect, lattice distortion effect, hysteresis band diffusion effect and cocktail effect, has excellent mechanical properties such as high strength, high hardness, corrosion resistance and wear resistance, and provides a new exploration direction for the research and development of novel high-temperature materials. In particular, the high Wen Gaoshang alloy is not limited by the application of a single principal element, and extends to the center position of a phase diagram in the selection of a component principal element, so that more possibilities are provided for the component design of the superalloy, and more solutions are provided for the problem of high density of the conventional superalloy. The development of a new generation of high Wen Gaoshang alloy with high temperature resistance, high strength and high toughness as a high-temperature structural material of an aeroengine has become an important link for promoting the development of the aerospace field. In recent years, the development of high Wen Gaoshang alloys has tended to have a multi-principal component FCC/L12 phase structure, which exhibits excellent high temperature comprehensive properties, but the alloy composition strengthened with L12 phase still contains 50% or more of nickel and cobalt elements, and the cost is high. On the basis of ensuring that the alloy has the characteristics of cost saving, light weight and high strength, the alloy still has good forming performance, and the requirement of subsequent forming and manufacturing is still the technical problem to be mainly solved in the prior art.
Disclosure of Invention
In view of the above, the invention provides a high Wen Gaoshang alloy and a preparation method thereof, and the high Wen Gaoshang alloy provided by the invention has the advantages of low application cost, light weight, improved high-temperature service performance of the alloy, and good hot forming processing capability.
The invention provides a high Wen Gaoshang alloy, which comprises the following elements in percentage by mass: 0.03 to 0.04wt.% of C, 4 to 5.5wt.% of W, 0.5 to 3.5wt.% of Nb, 2 to 4.5wt.% of Ti, 4 to 6wt.% of Mo, 5.5 to 8wt.% of Al, 16.5 to 19wt.% of Fe, 8 to 10wt.% of Cr, 19 to 22wt.% of Co, and the balance of Ni;
the mass ratio of Ti to Al is 0.25-0.82, the mass ratio of Ni/(Al+Ti) is 3+ -0.2, and the mass ratio of W/Mo is 0.67-1.22; .
The microstructure of the high-temperature high-entropy alloy in the as-cast state consists of gamma phase, gamma' phase and TiC.
Preferably, the volume fraction of the gamma' phase ranges from 46% to 64%, and the volume fraction of TiC ranges from 0.15% to 0.33%.
Preferably, the density of the high-temperature high-entropy alloy is less than 8g/cm 3
The invention provides a preparation method of the high-temperature high-entropy alloy, which comprises the following steps:
according to the element composition of the high-temperature high-entropy alloy, the alloy raw materials are subjected to vacuum induction smelting to obtain alloy liquid;
Cooling and solidifying the alloy liquid to obtain an alloy cast ingot;
remelting the alloy cast ingot, and cooling and solidifying the alloy liquid obtained by remelting again to obtain the high-temperature high-entropy alloy.
Preferably, the alloy raw material is subjected to vacuum induction melting, namely the alloy raw material is placed in a CaO crucible for vacuum induction melting.
Preferably, the vacuum induction melting has a vacuum degree of 5×10 -3 Pa～1×10 -2 Pa, wherein the vacuum induction smelting is performed in a shielding gas, and the pressure of the shielding gas is 0.1 Pa-0.3 Pa.
Preferably, the vacuum induction melting comprises:
the initial heating power is 2-3 kW, the heating power is increased to 12kW at the rate of 2-3 kW/10min, and the smelting temperature is 1550-1700 ℃;
and (3) preserving heat at the smelting temperature, wherein the time of preserving heat is 10-20 min.
Preferably, the purity of the alloy feedstock is higher than 99.9%.
Preferably, the alloy raw materials are respectively: the powder comprises W simple substance powder, nb simple substance particles, ti simple substance particles, mo simple substance particles, al simple substance particles, fe simple substance particles, cr simple substance particles, co simple substance particles, ni simple substance particles and WC powder.
The invention also provides application of the high-temperature high-entropy alloy or the high Wen Gaoshang alloy obtained by the preparation method in the technical scheme in preparation of the turbine disk.
The invention provides a high Wen Gaoshang alloy, which comprises the following elements in percentage by mass: :0.03 to 0.04wt.% of C, 4 to 5.5wt.% of W, 0.5 to 3.5wt.% of Nb, 2 to 4.5wt.% of Ti, 4 to 6wt.% of Mo, 5.5 to 8wt.% of Al, 16.5 to 19wt.% of Fe, 8 to 10wt.% of Cr, 19 to 22wt.% of Co, and the balance of Ni; the mass ratio of Ti/Al is 0.25-0.82, the mass ratio of Ni/(Al+Ti) is 3+/-0.2, and the mass ratio of W/Mo is 0.67-1.22; the method comprises the steps of carrying out a first treatment on the surface of the The microstructure of the high-temperature high-entropy alloy in the as-cast state consists of gamma phase, gamma' phase and TiC. In the present invention, ni, co and Fe elements are main elements of the conventional superalloy; cr and Al elements can form compact Cr at high temperature 2 O 3 And Al 2 O 3 An oxide layer, thereby imparting excellent oxidation resistance and hot corrosion resistance to the high Wen Gaoshang alloy; nb and Ti are L12 phase stabilizing elements, and the basic structure of the L12 phase is Ni 3 (Al, ti). In addition, al and Ti elements are called low-density elements, and when Ni/(al+ti) is close to 3, the alloy density is low and the high-temperature deformability is good. Based on the actions of the elements, ni, co, cr, fe, al, mo is taken as a main element, a small amount of Ti, nb, W, C elements are added into the high Wen Gaoshang alloy to form a solid solution gamma phase of a face-centered cubic (FCC) structure and a gamma 'phase of an ordered face-centered cubic (L12) structure, and the gamma' phase is uniformly distributed on a matrix gamma phase as a second phase strengthening phase. Meanwhile, the C element and the Ti element are combined to form TiC, the TiC is positioned at a crystal boundary, the effects of pinning dislocation and the crystal boundary are achieved, critical slitting stress is reduced, the binding force between dendrites of the alloy in an as-cast state is enhanced, diffusion of carbon and metal atoms is promoted, grain refinement and increase of the density of the crystal boundary are achieved, and the hardness and high-temperature compressive strength of the as-cast alloy are remarkably improved. The high Wen Gaoshang alloy with the cocktail effect is formed by adjusting the proportion of different alloy elements, and has good hot forming processing capacity on the premise of controlling low density, so that the large-size bar preparation of the novel low-density high-entropy high-temperature alloy and the large-size production requirement of the forming and manufacturing of parts with complex shapes are met, and the high-temperature-resistant alloy is suitable for high-temperature-resistant structural members such as turbine discs of space engines.
In addition, the Ni content in the high Wen Gaoshang alloy provided by the invention is lower than 50wt.%, so that the stacking fault energy of the alloy is reduced, and the potential applicability of the alloy is improved; the simultaneous existence of Cr, ni and Co elements avoids the formation of sigma phase and single FCC phase, and meets the good compression performance of the alloy at high temperature.
Furthermore, the CaO crucible is adopted in the preparation of the high-temperature high-entropy alloy, so that the content of impurity S, O element in the alloy is reduced, secondary oxidation is avoided, the components of the alloy are strictly controlled, the quality is stable, and the performance of the alloy is further ensured.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an XRD pattern of a high Wen Gaoshang alloy obtained in example 1 of the present invention;
FIG. 2 is an EBSD microstructure of the as-cast high temperature and high entropy alloy obtained in example 1 of the present invention;
FIG. 3 is a graph showing the compressive stress strain curves of test examples 1 to 4 according to the present invention;
FIG. 4 is a chart of EBSD microstructure according to test example 1 of the present invention;
FIG. 5 is an EBSD microstructure map of test example 2 according to the present invention;
FIG. 6 is an EBSD microstructure map of test example 3 according to the present invention;
FIG. 7 is an EBSD microstructure chart of test example 4 according to the present invention.
Detailed Description
The invention provides a high Wen Gaoshang alloy, which comprises the following elements in percentage by mass: :0.03 to 0.04wt.% of C, 4 to 5.5wt.% of W, 0.5 to 3.5wt.% of Nb, 2 to 4.5wt.% of Ti, 4 to 6wt.% of Mo, 5.5 to 8wt.% of Al, 16.5 to 19wt.% of Fe, 8 to 10wt.% of Cr, 19 to 22wt.% of Co, and the balance of Ni;
the mass ratio of Ti to Al is 0.25-0.82, the mass ratio of Ni/(Al+Ti) is 3+ -0.2, and the mass ratio of W/Mo is 0.67-1.22;
the microstructure of the high-temperature high-entropy alloy in the as-cast state consists of gamma phase, gamma' phase and TiC.
The high Wen Gaoshang alloys provided herein include 0.03 to 0.04wt.% C, which may be specifically 0.03 or 0.04wt.% in embodiments. In the invention, the addition of the element C can form TiC with Ti at the grain boundary, pin dislocation and the grain boundary, strengthen the bonding force between dendrites of the alloy in an as-cast state, and further greatly improve the high-temperature performance of the as-cast alloy.
The high Wen Gaoshang alloy provided by the invention comprises 2.5 to 3.5wt.% W, in embodiments may be specifically 4, 4.5, 5 or 5.5wt.% W, and in the invention the element W has the effect of increasing the mismatch stress in the gamma phase and decreasing the mismatch stress in the gamma' phase.
The high Wen Gaoshang alloys provided herein include 0.5 to 3.5wt.% Nb, which may be specifically 0.5, 1.0, 2.0, or 3.5wt.% Nb in embodiments. In the invention, nb element is solid solution strengthening element and is gamma ' phase stabilizing element with Ti element, which affects the degree of mismatching between gamma phase and gamma ' phase and improves the thermal stability of gamma ' phase. In the invention, when the Nb content is less than 0.5 wt%, the gamma' -phase content of the alloy is less and the plasticity is lower; at Nb contents exceeding 3.5wt%, the morphology of gamma' -phase changes from spherical and elliptical to square, and the plasticity and ductility decrease.
The high Wen Gaoshang alloys provided herein include 2 to 4.5wt.% Ti, which in embodiments may be specifically 2.0, 3.0, 3.5, or 4.5wt.% Ti. In the invention, ti element is helpful for improving the stable stacking fault energy of the alloy system, obviously reducing the adaptability of the system to surface defects, and inhibiting the precipitation of Laves phase under the combined action of Nb element, thereby improving the plasticity of the alloy. And the Ti element and the C element can form carbide TiC at the grain boundary to play a role of pinning, thereby achieving the purpose of strengthening crystallization. In the present invention, when the Ti content is less than 2.0wt.%, the volume fraction of the gamma' -phase formed in the alloy matrix is smaller and the strengthening effect is weaker; when the Ti content exceeds 4.5wt.%, the precipitation of η phase of a TCP (topologically close-packed) structure at grain boundaries is promoted in long-term aging, and the high-temperature stability of the alloy is lowered.
The high Wen Gaoshang alloys provided herein include 5.5 to 8wt.% Al, which may be specifically 5.5, 6.5, 7.0, or 8.0wt.% in embodiments. In the invention, al is a low-density element, which is helpful for improving the strength and hardness of the alloy; capable of forming dense Al at high temperature 2 O 3 The oxidation layer improves the high-temperature oxidation resistance and hot corrosion resistance of the alloy; combines with Ni and Ti element to form gamma' phase Ni 3 (Al, ti) and plays a role in strengthening a second phase. In the invention, the mass ratio of Ti/Al is 0.25-0.82, the distribution of the alloy element in gamma/gamma 'is directly influenced by the ratio of Ti/Al, and the distribution ratio of the alloy element in gamma'/gamma is deviated from 1 by the ratio of Ti/Al. In the invention, when the Ti/Al value is less than 0.25, the beta-NiAl phase is easy to be separated out from the matrix, thereby reducing the high-temperature durability of the alloy; when the Ti/Al value exceeds 0.82, eta-Ni is likely to precipitate in the matrix 3 Ti phase, reducing the structural stability of the alloy and greatly reducing the high-temperature strength of the alloy.
The high Wen Gaoshang alloy provided by the present invention includes 4 to 6wt.% Mo, which may be specifically 4, 4.5, 5.5, or 6wt.% in embodiments. In the present invention, the Mo element has an extremely strong solid solution strengthening effect. In the invention, the mass ratio of the W/Mo is 0.67-1.22, and the high W/Mo value can effectively avoid precipitation of harmful eta phases in grain boundaries and crystals under long-time working at high temperature. In the invention, eta phase is easy to be separated out from the matrix when the W/Mo value is less than 0.67, and the high-temperature durability of the alloy is reduced; when the W/Mo value exceeds 1.22, needle-like mu phase is easy to separate out in the matrix, the plasticity of the alloy is reduced, the notch sensitivity of the alloy is caused, the comprehensive mechanical property is deteriorated, and the high-temperature tissue stability of the alloy is reduced.
The high Wen Gaoshang alloys provided herein include 16.5 to 19wt.% Fe, which in embodiments may be specifically 16.5, 17, 17.5, 18, 18.5, or 19wt.%. In the invention, fe is a main matrix element of the high Wen Gaoshang alloy, has ferromagnetism, and is beneficial to improving the durability and the thermal stability of the alloy.
The high Wen Gaoshang alloys provided herein include 8 to 10 wt% Cr, which in embodiments may be specifically 8.0, 8.7, 9.2, or 10.0 wt%. In the present invention, cr is a high Wen Gaoshang alloyMain element, capable of forming dense Cr at high temperature 2 O 3 The oxidation layer improves the oxidation resistance and the hot corrosion resistance of the alloy.
The high Wen Gaoshang alloys provided herein include 19 to 22wt.% Co, which may be specifically 19.0, 20.0, 21.5, or 22wt.% in embodiments. In the invention, co is the main element of the alloy matrix, and the addition of Co reduces the stacking fault energy of the system, can enrich among dendrites, plays the role of an adhesive, is beneficial to improving the plasticity and toughness of the alloy and prevents the occurrence of brittle fracture during solidification.
The high Wen Gaoshang alloy provided by the invention comprises the balance of Ni, wherein the content of Ni in the alloy is lower than 50wt.%, specifically 28.17-31.76 wt.%, and the lower content of Ni element reduces the stacking fault energy of the alloy and expands the potential applicability of the alloy; in addition, under the simultaneous existence of Cr, co and Ni elements, the formation of sigma phase and single FCC phase is avoided, and the good compression performance of the alloy at high temperature is satisfied.
In the present invention, the mass ratio of Ni/(Al+Ti) is 3.+ -. 0.2, and the closer the mass ratio of Ni/(Al+Ti) is to 3, the larger the gamma' -phase volume fraction is. Because the mismatch degree of the gamma 'phase and the matrix gamma phase is high, the gamma' phase is a strengthening phase, and the compressive strength of the alloy is obviously improved.
The microstructure of the high Wen Gaoshang alloy provided by the invention in an as-cast state consists of a gamma phase, a gamma ' phase and TiC, wherein the gamma phase is a solid solution gamma phase of a face-centered cubic (FCC) structure, the gamma ' phase is an ordered face-centered cubic (L12) structure, and the gamma ' phase is uniformly distributed on a matrix gamma phase as a second phase strengthening phase. In the invention, the volume fraction of the gamma phase is preferably 36.57% -55.35%; the volume fraction of the gamma prime phase is preferably 46% to 64%, more preferably 63.1%; the volume fraction of TiC is preferably 0.15-0.33%.
In the invention, the volume fraction range of TiC is limited to 0.15-0.33%, the TiC is positioned at the grain boundary, dislocation and the grain boundary are pinned, the critical cutting stress is reduced, the binding force between dendrites of the alloy in an as-cast state is enhanced, the diffusion of carbon and metal atoms is promoted, the grain refinement and the increase of the density of the grain boundary are realized, and the hardness and the high-temperature compressive strength of the as-cast alloy are remarkably improved.
The above-mentioned individual elementsUnder the interaction of elements, the high Wen Gaoshang alloy provided by the invention has low density and good high-temperature deformability, and the density of the high-temperature high-entropy alloy is lower than 8g/cm 3 。
The invention also provides a preparation method of the high-temperature high-entropy alloy, which comprises the following steps:
according to the element composition of the high-temperature high-entropy alloy, the alloy raw materials are subjected to vacuum induction smelting to obtain alloy liquid;
cooling and solidifying the alloy liquid to obtain an alloy cast ingot;
remelting the alloy cast ingot, and cooling and solidifying the alloy liquid obtained by remelting again to obtain the high-temperature high-entropy alloy.
The invention is not particularly limited in the kind of the alloy raw material, and the elemental materials or intermediate alloys of the above elements, which are well known to those skilled in the art, may be used; the preferred C source materials are carbide materials WC of C and W. Specifically, in the embodiment of the present invention, the elemental materials of W, nb, ti, mo, al, fe, cr, co and Ni are elemental powders or elemental particles of each element, and the carbide material WC is carbide powder or carbide particles. In the present invention, the purity of the alloy raw materials is preferably higher than 99.9%; the raw materials of each element are respectively as follows: the powder comprises W simple substance powder, nb simple substance particles, ti simple substance particles, mo simple substance particles, al simple substance particles, fe simple substance particles, cr simple substance particles, co simple substance particles, ni simple substance particles and WC powder. In the present invention, the particle size of the raw material powder is preferably 300 mesh; the particle size of the elementary particles is preferably
The alloy raw material is subjected to vacuum induction smelting to obtain alloy liquid. The apparatus for vacuum induction melting is not particularly limited, and a vacuum induction melting furnace well known to those skilled in the art may be used. According to the invention, the alloy raw material is preferably placed in the CaO crucible for vacuum induction melting, the content of impurity S, O element in the alloy is reduced by using the CaO crucible, secondary oxidation is avoided, the components of the alloy are strictly controlled, the quality is stable, and the performance of the alloy is further ensured. In the present invention, al and Ti raw materials are added through a hopper after all alloys except Al and Ti elements are melted.
In the present invention, the vacuum induction melting is preferably:
vacuumizing a vacuum bin of the vacuum induction smelting furnace, and then filling protective gas;
heating to the smelting temperature until the alloy raw materials are completely melted, and obtaining alloy liquid.
In the present invention, the vacuum degree of the vacuum induction melting is preferably 5×10 -3 Pa～1×10 -2 Pa, may be specifically 5×10 -3 、6×10 -3 、7×10 -3 、8×10 -3 、9×10 -3 Or 1X 10 -2 Pa; the protective gas is preferably high-purity argon, and the purity of the protective gas is preferably 99.999%; the pressure of the shielding gas is preferably 0.1Pa to 0.3Pa, and may specifically be 0.1, 0.2, or 0.3Pa.
In the present invention, the program for raising the temperature to the melting temperature is preferably:
the initial heating power is 2-3 kW, the heating power is increased to 12kW at the rate of 2-3 kW/10min, and the smelting temperature is 1550-1700 ℃;
and (3) preserving heat at the smelting temperature, wherein the time of preserving heat is 10-20 min.
In the present invention, the initial heating power may be specifically 2, 2.5 or 3kW, and the heating rate may be specifically 2, 2.5 or 3kW/10min; the smelting temperature may be in particular 1550, 1600, 1650 or 1700 ℃; the time of the heat preservation can be specifically 10, 15 or 20min, and the heat preservation ensures that the temperature and the components of the alloy liquid are uniform.
After the alloy liquid is obtained, the alloy liquid is cooled and solidified, and the alloy is cast. In the present invention, the condensation solidification is preferably natural cooling to room temperature.
After the alloy ingot is obtained, the alloy ingot is preferably remelted to obtain remelted alloy liquid; and cooling and solidifying the remelted alloy liquid again to obtain the high-temperature high-entropy alloy liquid. In the present invention, the remelting and recooling solidification scheme is preferably identical to the vacuum induction melting and cooling solidification scheme described in the above technical scheme, and will not be described herein.
In the present invention, the number of remelting and re-cooling solidification is preferably 1 to 2.
The high Wen Gaoshang alloy provided by the invention has a cocktail effect, has excellent high-temperature deformation performance under low density, and is suitable for high-temperature-resistant structural members such as a turbine disk of an aerospace engine.
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings.
It should be noted that, without conflict, the following embodiments and features in the embodiments may be combined with each other; and, based on the embodiments in this disclosure, all other embodiments that may be made by one of ordinary skill in the art without inventive effort are within the scope of the present disclosure.
It is noted that various aspects of the embodiments are described below within the scope of the following claims. It should be apparent that the aspects described herein may be embodied in a wide variety of forms and that any specific structure and/or function described herein is merely illustrative. Based on the present disclosure, one skilled in the art will appreciate that one aspect described herein may be implemented independently of any other aspect, and that two or more of these aspects may be combined in various ways. For example, an apparatus may be implemented and/or a method practiced using any number of the aspects set forth herein. In addition, such apparatus may be implemented and/or such methods practiced using other structure and/or functionality in addition to one or more of the aspects set forth herein.
Example 1
A Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy consists of the following elements in percentage by mass: c:0.03wt.%, W:5.5wt.%, nb:2wt.% Ti:4.5wt.% Mo:4.5wt.% Al:5.5wt.% Fe:16.5wt.%, cr:8wt.%, co:21.5wt.% Ni: the balance; ti/al=0.82, ni/(al+ti) =3.197, w/mo=1.22.
The preparation method of the Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy comprises the following steps:
(1) Weighing the required WC intermediate alloy, the W simple substance, the Nb simple substance, the Ti simple substance, the Mo simple substance, the Al simple substance, the Fe simple substance, the Cr simple substance, the Co simple substance and the Ni simple substance according to the element component proportion, mixing and putting the mixture into a CaO crucible of a vacuum induction melting furnace, wherein active elements Al and Ti are added through a hopper after all other element raw materials are melted;
(2) After the raw materials are placed in a vacuum induction smelting furnace, the vacuum bin is vacuumized to 8 multiplied by 10 -3 Pa, and then filling high-purity Ar with the purity of 99.999 percent to maintain the pressure of the vacuum bin to be 0.2Pa;
(3) The initial heating power is 2kW, 2kW is increased every 10min, after the heating power is increased to 12kW, the smelting temperature reaches 1600 ℃, and the furnace burden is completely melted to obtain molten alloy;
(4) Preserving the temperature of the alloy liquid at 1600 ℃ for 10min to ensure that the temperature and the components of the alloy liquid are uniform, stopping heating and preserving the temperature, and naturally cooling and solidifying in a crucible to obtain an alloy cast ingot;
(5) Repeating the step (3) for remelting and then repeating the step (4) for cooling and solidifying;
(6) Repeating the step (5) for 1 time to obtain the high Wen Gaoshang alloy.
XRD detection is carried out on the obtained high Wen Gaoshang alloy, and the result is shown in FIG. 1e, and as can be seen from FIG. 1e, the as-cast alloy mainly comprises gamma phase, gamma' phase and a small amount of TiC;
the obtained high Wen Gaoshang alloy is subjected to EBSD microstructure analysis, and the result is shown in figure 2, and as can be seen from figure 2, the microstructure of the as-cast alloy consists of gamma phase, gamma 'phase and TiC, wherein the gamma' phase accounts for 63.1%, and the TiC accounts for 0.33%; gamma phase is matrix phase, belongs to a face-centered stereo FCC structure, and has typical lattice parameter a= 0.3616nm; the gamma' phase is an ordered face-centered cubic L12 structure, and the typical lattice parameter a= 0.3605nm has the characteristics of uniform dispersion nucleation, coherent lattice, low phase interface energy, high stability and the like.
The hardness of the obtained high Wen Gaoshang alloy was measured by using a THV-1MDT type micro Vickers hardness tester with a test force of 1kgf, at least 3 effective hardness data were measured for each sample, and the average hardness value was calculated to be 528HV1.
The density of the resulting high Wen Gaoshang alloy was measured 3 times per sample using an archimedes drainage method with an average density value of 7.84g/cm 2 。
The thermal expansion coefficient is measured by a DIL805A thermal expansion rapid phase-change meter, and the measuring range is 25-800 ℃ and 25-900 ℃. The expansion curve of the sample length L with temperature T was measured by first rapidly heating to around the test temperature at a rate of 50 ℃/min and then slowly heating up at a rate of 10 ℃/min. Measuring 3 times, taking average value, linear expansion coefficient alpha 25～800℃ ＝14.23、α 25～900℃ ＝15.04。
Comparative examples 1 to 2
A high Wen Gaoshang alloy was prepared according to the procedure of example 1, except that the CaO crucible of example 1 was replaced by an Al2O3 crucible or an MgO crucible.
The elemental N, S and O in the resulting high Wen Gaoshang alloy were measured and the results are shown in table 1.
Table 1 comparison of O, N, S content (ppm) in the high Wen Gaoshang alloys obtained in example 1 and comparative examples 1-2
| Crucible pot | O(ppm) | N(ppm) | S(ppm) |
| Al 2 O 3 | 13 | 9 | 28 |
| CaO | 6 | 3 | 22 |
| MgO | 15 | 13 | 30 |
Test example 1-1
A high Wen Gaoshang alloy obtained in example 1 was subjected to a high Wen Zhun static compression test using a Gleeble 3800D thermal simulation tester, with a deformation amount set to 60%. To prevent oxidation of the samples, the experiments were performed in a vacuum environment. The compressed sample size was a cylindrical bar-shaped sample (sample diameter 10mm, height 15 mm) with an aspect ratio selected to be 1.5. The test temperature is 900 ℃, and after the sample is heated to 900 ℃ and kept for 10min, the temperature is kept constant by 1X 10 -3 ·s -1 Compression experiments were performed at the strain rate of (c).
The compressive stress strain curve is shown in FIG. 3, and the compressive strength is 174MPa;
as a result of XRD phase analysis of the compressed sample, as shown in fig. 1d, compared with the as-cast alloy of example 1, the phase type is unchanged, and the sample still comprises gamma phase, gamma ' phase and TiC, the diffraction peak value of the gamma phase matrix is reduced, the diffraction peak value of the gamma ' phase is increased, but the diffraction peak value of the gamma phase is still higher than the diffraction peak value of the gamma ' phase;
the compressed sample was subjected to microscopic observation by EBSD, as shown in fig. 4, in which the dynamic recrystallization structure (blue position) volume fraction was 34.3%, the subgrain structure (yellow position) volume fraction was 37.6%, and the deformed structure (red position) volume fraction was 28.1%.
Test examples 1 to 2
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in example 1 in accordance with the method of test example 1-1, with the difference thatIn that the strain rate is changed to be constant 1X 10 -2 ·s -1 Compression experiments were performed at the strain rate of (c).
The compressive stress strain curve is shown in FIG. 3, and the compressive strength is 296MPa;
as shown in fig. 1c, compared with the uncompressed and test 1, the sample after compression is subjected to XRD phase analysis, and the phase types are consistent and still consist of gamma phase, gamma ' phase and TiC, but the diffraction peak value of the gamma ' phase is slightly higher than that of the gamma phase, and a new low-intensity gamma ' phase diffraction peak appears;
The compressed sample was subjected to microscopic observation by EBSD, as shown in fig. 5, in which the dynamic recrystallization structure (blue position) volume fraction was 20.3%, the subgrain structure (yellow position) volume fraction was 20.5%, and the deformed structure (red position) volume fraction was 59.2%. The recrystallized structure and the subgrain structure were decreased and the deformed structure was increased as compared with test example 1.
Test examples 1 to 3
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in example 1 in accordance with test example 1-1, except that the strain rate was changed to be constant 1X 10 -1 ·s -1 Compression experiments were performed at the strain rate of (c).
The compressive stress strain curve is shown in FIG. 3, and the compressive strength is 439MPa;
XRD phase analysis was performed on the compressed sample, and as a result, as shown in FIG. 1b, compared with the uncompressed sample and the sample 1-2, the sample consisted of gamma phase, gamma 'phase and TiC, the intensity of the gamma' phase diffraction peak was increased relative to the intensity of the gamma phase diffraction peak, and the ratio was about 1.51;
the compressed sample was subjected to microscopic observation by EBSD, as shown in fig. 6, in which the dynamic recrystallization structure (blue position) volume fraction was 9.4%, the subgrain structure (yellow position) volume fraction was 16.2%, and the deformed structure (red position) volume fraction was 74.4%. The recrystallized and sub-crystalline structures were reduced compared to test examples 1-2, and the volume fraction of recrystallized structure/volume fraction of sub-crystalline was about 0.58, with a ratio of less than 1, no longer tending to be equal.
Test examples 1 to 4
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in example 1 in accordance with test example 1-1, except that the strain rate was changed to be constant for 1s -1 Compression experiments were performed at the strain rate of (c).
The compressive stress strain curve is shown in FIG. 3, and the compressive strength is 520MPa;
XRD phase analysis was performed on the compressed sample, and as a result, as shown in FIG. 1a, the sample still consisted of gamma phase, gamma 'phase and TiC, and the diffraction peak intensities of gamma' phase and gamma phase were further increased, but the ratio was still about 1.51, as compared with the uncompressed samples 1-3;
the compressed sample was subjected to microscopic observation by EBSD, as shown in fig. 7, in which the dynamic recrystallization structure (blue position) volume fraction was 6.99%, the subgrain structure (yellow position) volume fraction was 16.9%, and the deformed structure (red position) volume fraction was 76.1%. The recrystallized and sub-crystalline structures were further reduced compared to test examples 1-3, with the recrystallized structure volume fraction/sub-crystalline volume fraction being about 0.41, the ratio being less than 0.5, the difference being more than half.
Example 2
A Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy consists of the following elements in percentage by mass: c:0.04wt.%, W:4wt.%, nb:1wt.% Ti:2wt.% Mo:6wt.% Al:8wt.%, fe:18.5wt.%, cr:10wt.%, co:20wt.%, ni: the balance; ti/al=0.25, ni/(al+ti) =3.046, w/mo=0.67.
The Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy with the composition of the embodiment is prepared according to the scheme of the embodiment 1, wherein the difference is that: in this example, the initial power was 3kW, the rate was 3kW/10min, the melting temperature was 1700℃and the holding time was 20min.
XRD detection is carried out on the obtained as-cast high-temperature high-entropy alloy to obtain a result similar to that of the embodiment 1, wherein the as-cast alloy mainly comprises gamma phase, gamma' phase and a small amount of TiC;
EBSD microstructure analysis is carried out on the obtained as-cast high-temperature high-entropy alloy, and the result shows that the alloy microstructure consists of gamma phase, gamma ' phase and TiC, the volume fraction of the gamma ' phase is 46.5%, the ratio of gamma '/gamma volume fraction is 0.9, and the TiC accounts for 0.15%.
The obtained as-cast high-temperature high-entropy alloy was subjected to hardness, density and thermal expansion coefficient tests, respectively, in the same manner as in example 1, and an average hardness value of 542HV1 and an average density value of 7.69g/cm was calculated 2 Average linear expansion coefficient alpha 25～800℃ ＝14.57、α 25～900℃ ＝15.51。
Test example 2-1
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in example 2 in the manner of test example 1-1 to obtain a high value of 0.001s as shown in FIG. 3 -1 Results with similar curves show that the compressive strength is 102MPa;
XRD phase analysis is carried out on the compressed sample, the phase types and the diffraction peak numbers are similar to those of the test example 1-1, the sample still comprises gamma phase, gamma 'phase and TiC, and the diffraction peak value of the gamma phase is higher than that of the gamma' phase;
The compressed sample was observed by EBSD and the microstructure consisted of a dynamic recrystallization structure, a sub-crystalline structure and a deformed structure, with volume fractions of 39.6%, 43.9% and 16.5%, respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with test example 1-1.
Test example 2-2
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in example 2 in accordance with the methods of test examples 1-4 to obtain a high value of 1s as shown in FIG. 3 -1 The result of the similar curve is that the compressive strength is 306MPa;
XRD phase analysis is carried out on the compressed sample, the phase types and the diffraction peak numbers are similar to those of the test examples 1-4, the sample still comprises gamma phase, gamma 'phase and TiC, the diffraction peak value of the gamma phase is obviously higher than that of the gamma' phase, and the ratio is about 1.3;
the compressed sample was observed by EBSD and the microstructure consisted of a dynamic recrystallization structure, a sub-crystalline structure and a deformed structure, with volume fractions of 20.3%, 22.4% and 57.3%, respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with test examples 1 to 4.
Example 3
A Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy consists of the following elements in percentage by mass: c:0.03wt.%, W:4.5wt.%, nb:3.5wt.%, ti:3.5wt.% Mo:4wt.% Al:6.3wt.% Fe:19wt.%, cr:8.7wt.%, co:22wt.%, ni: the balance; ti/al=0.56, ni/(al+ti) =2.905, w/mo=1.125.
The Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy with the composition of the embodiment is prepared according to the scheme of the embodiment 1, wherein the difference is that: in the embodiment, the smelting temperature is 1550 ℃ and the heat preservation time is 20min.
XRD detection is carried out on the obtained as-cast high-temperature high-entropy alloy to obtain a result similar to that of the embodiment 1, wherein the as-cast alloy mainly comprises gamma phase, gamma' phase and a small amount of TiC;
EBSD microstructure analysis is carried out on the obtained as-cast high-temperature high-entropy alloy, and the result shows that the alloy microstructure consists of gamma phase, gamma ' phase and TiC, the volume fraction of the gamma ' phase is 55.3%, the ratio of gamma '/gamma volume fraction is 1.2, and the TiC accounts for 0.28%.
The obtained as-cast high-temperature high-entropy alloy was subjected to hardness, density and thermal expansion coefficient tests, respectively, in the same manner as in example 1, and an average hardness value of 514HV1 and an average density value of 7.79g/cm was calculated 2 Average linear expansion coefficient alpha 25～800℃ ＝14.38、α 25～900℃ ＝15.32。
Test example 3-1
A high Wen Zhun static compression test was conducted on the high Wen Gaoshang alloy obtained in example 3 in accordance with the method of test example 1-1 to obtain a high value of 0.001s as shown in FIG. 3 -1 Results with similar curves show that the compressive strength is 135MPa;
XRD phase analysis is carried out on the compressed sample, the phase types and the diffraction peak numbers are similar to those of the test example 1-1, the sample still comprises gamma phase, gamma 'phase and TiC, and the diffraction peak value of the gamma' phase is slightly higher than that of the gamma phase;
The compressed sample was observed by EBSD and the microstructure consisted of a dynamic recrystallization structure, a sub-crystalline structure and a deformed structure, with volume fractions of 38.0%, 40.2% and 21.8%, respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with test example 1-1.
Test example 3-2
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in example 3 in accordance with the methods of test examples 1-4 to obtain a high alloy equivalent to 1s in FIG. 3 -1 The result of the similar curve is that the compressive strength is 415MPa;
XRD phase analysis is carried out on the compressed sample, the types of phases and the number of diffraction peaks are similar to those of the test examples 1-4, the sample still comprises gamma phase, gamma 'phase and TiC, and the diffraction peak value of the gamma' phase is almost equal to that of the gamma phase;
the compressed sample was observed by EBSD and the microstructure consisted of a dynamic recrystallization structure, a sub-crystalline structure and a deformed structure, with volume fractions of 18.9%, 23.8% and 57.3%, respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with test examples 1 to 4.
Example 4
A Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy consists of the following elements in percentage by mass: c:0.04wt.%, W:5wt.%, nb:0.5wt.%, ti:2.8wt.% Mo:5.5wt.% Al:7.6wt.% Fe:17.5wt.%, cr:9.2wt.%, co:19wt.%, ni: the balance; ti/al=0.37, ni/(al+ti) =3.16, w/mo=0.91.
The Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy with the composition of the embodiment is prepared according to the scheme of the embodiment 1, wherein the difference is that: in this example, the initial power was 3kW, the rate was 3kW/10min, and the incubation time was 15min.
XRD detection is carried out on the obtained as-cast high-temperature high-entropy alloy to obtain a result similar to that of the embodiment 1, wherein the as-cast alloy mainly comprises gamma phase, gamma' phase and a small amount of TiC;
EBSD microstructure analysis is carried out on the obtained as-cast high-temperature high-entropy alloy, and the result shows that the alloy microstructure consists of gamma phase, gamma ' phase and TiC, the volume fraction of the gamma ' phase is 51.8%, the ratio of gamma '/gamma volume fraction is 1.1, and the TiC ratio is 0.27%.
For the obtained as-cast high temperatureThe high-entropy alloy was subjected to hardness, density and thermal expansion coefficient tests, respectively, using the same procedure as in example 1, and calculated to give an average hardness value of 527HV1 and an average density value of 7.73g/cm 2 Average linear expansion coefficient alpha 25～800℃ ＝14.46、α 25～900℃ ＝15.39。
Test example 4-1
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in example 4 in the manner of test example 1-1 to obtain a high value of 0.001s as shown in FIG. 3 -1 The result of the similar curve is that the compressive strength is 127MPa;
XRD phase analysis is carried out on the compressed sample, the phase types and the diffraction peak numbers are similar to those of the test example 1-1, the sample still comprises gamma phase, gamma 'phase and TiC, and the diffraction peak value of the gamma' phase is slightly lower than that of the gamma phase;
The compressed sample was observed by EBSD and the microstructure consisted of a dynamic recrystallization structure, a sub-crystalline structure and a deformed structure, with volume fractions of 38.4%, 41.1% and 20.5%, respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with test example 1-1.
Test example 4-2
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in example 4 in accordance with the methods of test examples 1-4 to obtain a high value of 1s as shown in FIG. 3 -1 Results with similar curves show that the compressive strength is 381MPa;
XRD phase analysis is carried out on the compressed sample, the phase types and the diffraction peak numbers are similar to those of the test examples 1-4, the sample still comprises gamma phase, gamma 'phase and TiC, the diffraction peak value of the gamma' phase is lower than that of the gamma phase, and the ratio is about 0.94;
and (3) carrying out microscopic structure observation on the compressed sample by utilizing EBSD, wherein the microscopic structure consists of a dynamic recrystallization structure, a sub-crystal structure and a deformation structure, and the volume fractions are 17.3%, 19.2% and 63.5% respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with test examples 1 to 4.
Comparative example 3
A Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy consists of the following elements in percentage by mass: c:0.04wt.%, W:3.5wt.%, nb:0.5wt.%, ti:6wt.% Mo:5.5wt.% Al:4wt.% Fe:16.5wt.%, cr:10wt.%, co:19wt.%, ni: the balance; ti/al=1.5, ni/(al+ti) =3.496, w/mo=0.636.
Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy with the composition of the comparative example was prepared according to the method of example 1.
XRD detection is carried out on the obtained as-cast high-temperature high-entropy alloy, and the result shows that the as-cast alloy consists of gamma phase, gamma' phase, eta phase and TiC;
EBSD microstructure analysis is carried out on the obtained as-cast high-temperature high-entropy alloy, and the result shows that the alloy microstructure mainly comprises gamma/gamma ' two phases, the volume fraction of the gamma ' phase is 35.7%, and the ratio of gamma '/gamma volume fraction is 0.6.
The obtained as-cast high-temperature high-entropy alloy was subjected to hardness, density and thermal expansion coefficient tests, respectively, in the same manner as in example 1, and the average hardness value was 476HV1 and the average density value was 8.32g/cm 2 Average linear expansion coefficient alpha 25～800℃ ＝14.75、α 25～900℃ ＝15.83。
Comparative test example 3-1
A high Wen Zhun static compression test was conducted on the high Wen Gaoshang alloy obtained in comparative example 3 in accordance with the method of test example 1-1, with the compressive stress strain curve having a trend of 0.001s in FIG. 3 -1 The curves are similar, and the compressive strength is 83MPa;
XRD phase analysis is carried out on the compressed sample, the phase consists of gamma phase, gamma 'phase, eta phase and TiC, and the diffraction peak value of the gamma' phase is obviously lower than that of the gamma phase;
the compressed sample was observed by EBSD and the microstructure consisted of a dynamic recrystallization structure, a sub-crystalline structure and a deformed structure, with volume fractions of 42.4%, 44.2% and 13.4%, respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with test examples 1-1, 2-1, 3-1 and 4-1.
Comparative test example 3-2
According to the method of test examples 1 to 4A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in comparative example 3, with the compressive stress strain curve trend corresponding to 1s in FIG. 3 - The curves are similar, and the compressive strength is 278MPa;
XRD phase analysis is carried out on the compressed sample, the phase consists of gamma phase, gamma 'phase, eta phase and TiC, the diffraction peak value of the gamma' phase is obviously lower than that of the gamma phase, and the ratio is only about 0.52;
and (3) carrying out microscopic structure observation on the compressed sample by utilizing EBSD, wherein the microscopic structure consists of a dynamic recrystallization structure, a sub-crystal structure and a deformation structure, and the volume fractions are respectively 22.1%, 23.6% and 54.3%. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with the test examples 1-4, 2-2, 3-2 and 4-2.
Comparative example 4
A Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy consists of the following elements in percentage by mass: c:0.03wt.%, W:2wt.%, nb:1wt.% Ti:2wt.% Mo:4wt.% Al:8.5wt.% Fe:20.5wt.%, cr:11wt.%, co:23wt.%, ni: the balance; ti/al=0.235, ni/(al+ti) =2.66, w/mo=0.5.
Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy with the composition of the comparative example was prepared according to the method of example 1.
XRD detection is carried out on the obtained as-cast high-temperature high-entropy alloy, and the result shows that the as-cast alloy consists of gamma phase, gamma' phase, beta phase and TiC;
EBSD microstructure analysis is carried out on the obtained as-cast high-temperature high-entropy alloy, and the result shows that the alloy microstructure mainly comprises gamma/gamma ' two phases, the volume fraction of the gamma ' phase is 40.2%, and the ratio of gamma '/gamma volume fraction is 0.67.
The obtained as-cast high-temperature high-entropy alloy was subjected to hardness, density and thermal expansion coefficient tests, respectively, in the same manner as in example 1, and an average hardness value of 510HV1 and an average density value of 8.04g/cm was calculated 2 Average linear expansion coefficient alpha 25～800℃ ＝14.63、α 25～900℃ ＝15.62。
Comparative test example 4-1
A high Wen Zhun static compression test was conducted on the high Wen Gaoshang alloy obtained in comparative example 4 in the manner of test example 1-1, with the compressive stress strain curve varying from 0.001s in FIG. 3 -1 The curves are similar, and the compressive strength is 96MPa;
XRD phase analysis is carried out on the compressed sample, the phase consists of gamma phase, gamma 'phase, beta phase and TiC, and the diffraction peak value of the gamma' phase is obviously lower than that of the gamma phase;
the compressed sample was observed by EBSD and the microstructure consisted of a dynamic recrystallization structure, a sub-crystalline structure and a deformed structure, with volume fractions of 41.3%, 42.8% and 15.9%, respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with test examples 1-1, 2-1, 3-1 and 4-1.
Comparative test example 4-2
A high Wen Zhun static compression test was performed on the high Wen Gaoshang alloy obtained in comparative example 4 in accordance with the methods of test examples 1-4, with the compressive stress strain curve trend corresponding to 1s in FIG. 3 - The curves are similar, and the compressive strength is 291MPa;
XRD phase analysis is carried out on the compressed sample, the phase consists of gamma phase, gamma 'phase, beta phase and TiC, the diffraction peak value of the gamma' phase is obviously lower than that of the gamma phase, and the ratio is only about 0.74;
and (3) carrying out microscopic structure observation on the compressed sample by utilizing EBSD, wherein the microscopic structure consists of a dynamic recrystallization structure, a sub-crystal structure and a deformation structure, and the volume fractions are 21%, 22.1% and 56.9% respectively. The recrystallized structure and the subgrain structure were increased and the deformed structure was decreased as compared with the test examples 1-4, 2-2, 3-2 and 4-2.
As can be seen from the results of comparative examples 1, 3 and 4, the variation of the mass fraction ratio of Ti/Al to Ni/(Al+Ti) affects the volume fraction of the gamma prime phase in the alloy. The gamma' -phase inhibits the recrystallization behavior, reduces the mass fraction of the recrystallized structure in plastic deformation, and improves the compressive strength thereof.
As can be seen from the above examples, the Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy provided by the invention has a high deformation temperature Degree t=900 ℃, at different strain rates (1×10 -3 s -1 ～1s -1 ) As can be seen from comparison with as-cast alloy, the alloy has good structural stability in the thermal deformation process, always keeps an FCC/L12 phase structure, and does not undergo solid solution phase transformation, namely, second phase gamma' phase strengthening is realized on a gamma phase solid solution matrix; the evolution process of the novel Ni-Co-Cr-Fe-Al-Mo high-temperature high-entropy alloy thermal deformation microstructure of the FCC/L12 phase structure mainly comprises a substructure and an original deformation structure formed by dynamic recrystallization and dislocation motion induction. Not only ensure the density to be lower than 8g/cm 3 Realizes low-cost control, has excellent high-temperature compression performance, can be suitable for high temperature resistant structural member application.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the scope of the present invention should be included in the present invention. Therefore, the protection scope of the invention is subject to the protection scope of the claims.
Claims (10)
1. A high Wen Gaoshang alloy, which comprises the following elements in percentage by mass: :0.03 to 0.04wt.% of C, 4 to 5.5wt.% of W, 0.5 to 3.5wt.% of Nb, 2 to 4.5wt.% of Ti, 4 to 6wt.% of Mo, 5.5 to 8wt.% of Al, 16.5 to 19wt.% of Fe, 8 to 10wt.% of Cr, 19 to 22wt.% of Co, and the balance of Ni;
The mass ratio of Ti to Al is 0.25-0.82, the mass ratio of Ni/(Al+Ti) is 3+ -0.2, and the mass ratio of W/Mo is 0.67-1.22; the method comprises the steps of carrying out a first treatment on the surface of the
The microstructure of the high-temperature high-entropy alloy in the as-cast state consists of gamma phase, gamma' phase and TiC.
2. The high Wen Gaoshang alloy of claim 1, wherein the gamma prime phase comprises a volume fraction in the range of 46% to 64% and the TiC comprises a volume fraction in the range of 0.15% to 0.33%.
3. The high temperature and high temperature according to claim 1 or 2An entropy alloy characterized in that the density of the high-temperature high-entropy alloy is less than 8g/cm 3 。
4. A method for producing the high-temperature high-entropy alloy according to any one of claims 1 to 3, comprising the steps of:
according to the element composition of the high-temperature high-entropy alloy of any one of claims 1 to 3, alloy raw materials are subjected to vacuum induction smelting to obtain alloy liquid;
cooling and solidifying the alloy liquid to obtain an alloy cast ingot;
remelting the alloy cast ingot, and cooling and solidifying the alloy liquid obtained by remelting again to obtain the high-temperature high-entropy alloy.
5. The method according to claim 3, wherein the vacuum induction melting of the alloy raw material is performed by placing the alloy raw material in a CaO crucible.
6. The method according to claim 4 or 5, wherein the vacuum induction melting has a vacuum degree of 5 x 10 -3 Pa～1×10 -2 Pa, wherein the vacuum induction smelting is performed in a shielding gas, and the pressure of the shielding gas is 0.1 Pa-0.3 Pa.
7. The method of manufacturing according to claim 4 or 5, characterized in that the vacuum induction melting comprises:
the initial heating power is 2-3 kW, the heating power is increased to 12kW at the rate of 2-3 kW/10min, and the smelting temperature is 1550-1700 ℃;
and (3) preserving heat at the smelting temperature, wherein the time of preserving heat is 10-20 min.
8. The method of claim 4, wherein the alloy feedstock has a purity of greater than 99.9%.
9. The method according to claim 4 or 8, wherein the alloy raw materials are respectively: the powder comprises W simple substance powder, nb simple substance particles, ti simple substance particles, mo simple substance particles, al simple substance particles, fe simple substance particles, cr simple substance particles, co simple substance particles, ni simple substance particles and WC powder.
10. Use of the high temperature high entropy alloy according to any one of claims 1 to 3 or the high Wen Gaoshang alloy obtained by the method according to any one of claims 4 to 9 in the manufacture of a turbine disk.
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